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Methyl iodide → HCID 178489511、化合物

HRID 447915
ノート
印刷プレビュー

反応式

HRID 447915 の反応式
[S:1]1[CH:5]=[CH:4][N:3]=[C:2]1[NH:6][C:7]([NH2:9])=S.CI.[CH3:12][O:13][C:14]1[CH:21]=[CH:20][CH:19]=[CH:18][C:15]=1[CH2:16][NH2:17]>CO.C(O)C>[CH3:12][O:13][C:14]1[CH:21]=[CH:20][CH:19]=[CH:18][C:15]=1[CH2:16][NH:17][C:7]([NH:6][C:2]1[S:1][CH:5]=[CH:4][N:3]=1)=[NH:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 812922-MethoxybenzylamineHCID 27710081,3-Thiazol-2-ylthiourea

生成物 1

HCID 178489511HCID 178489511、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

400 mg (2.51 mmol) N-1,3-thiazole-2-yl-thiourea were suspended in 20 ml of methanol and 392 mg (2.76 mmol) methyl iodide were added. The reaction mixture was stirred for 4 hours at reflux. Following removal of the solvent by vacuum distillation, the residue obtained was dissolved in 20 ml ethanol, 1.72 g (12.6 mmol) 2-methoxybenzylamine were added and the mixture was stirred for 20 hours at reflux. The solvent was removed on the rotovap. The residue was separated by preparative HPLC(RP-18 column, eluent water/acetonitrile/0.1% acetic acid) and 380 mg N-(2-methoxybenzyl)-N′-1,3-thiazole-2-ylguanidine were obtained.

後処理

  1. temperatureat reflux
  2. customremoval of the solvent
  3. distillationby vacuum distillation
  4. customthe residue obtained
  5. stirringthe mixture was stirred for 20 hours
  6. temperatureat reflux
  7. customThe solvent was removed on the rotovap
  8. customThe residue was separated by preparative HPLC(RP-18 column, eluent water/acetonitrile/0.1% acetic acid) and 380 mg N-(2-methoxybenzyl)-N′-1,3-thiazole-2-ylguanidine
  9. customwere obtained

出典と根拠

ORDレコード
ord-3fe931c8d63c4fc9b5137f254da77758
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08481576B2

反応ノート

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